Back to the Newsletters
eurostar-science homepage

NEWSLETTER OF eurostar-science

NO 2 -- October 14, 2001


           Erwin Marti, President

2.2 NEWS @
           Election of the new Board of Directors
           PhandTA 6
           New services @ the website

2.3 Highlights of the Conference on "Thermal Analysis and Material Science" in Munich
           Erwin Marti

2.4 Our Sponsors.Thermometric
           Dan Forsström


      Erwin Marti, President

The world has changed on September 11, 2001 from one minute to the next. We all are shocked about the human tragedies which occured when thousands of innocent people died. Today we are by far not yet aware of all the incisive and small consequences that will affect our future.

The crash of the Swiss airline triggered by this desaster and a last consequence of catastrophic Swissair management over at least ten years is one example shaking up many of us in the middle of Europe who grown up with the crossbow as a symbol for the Swiss Quality. But now it also appears as a sign that it seems to be high time for a restart of old traditional industries. We have to remember at any level - in industry, research and development - among other things not to overshoot in hazardous developments or to neglect the base of the literature, to work together in teams and make available all the scientific knowledge necessary to achieve a selected goal taking part in a network within the own scientific and working area.
eurostar-science offers such possibilities in the area of Physical Chemistry. So take the chance and participate in our activities.

Based on the previous structure of being an umbrella organization of National Societies which has now completely be changed into a Society with only personal membership, the number of members is currently still growing. Interested scientists are always welcome. eurostar-science is in contact over a network with about 1000 scientists, students and postdoctoral researcher mainly from Europe. The two main segments are scientists from universities and institutes, and employees of the pharmaceutical industry. Additionally our contacts are further enlarged with scientific coworkers of several manufacturers of instruments.
The scientific domains which are anticipated by our Society are Physical Chemistry applied to Pharmacy, Plant Protection, Fine Chemicals and Food Sciences.

All our activities are announced and reported on our website whereas proposals and scientific contributions are highly appreciated. Currently our main activity is the organization of PhandTA 6 and the workshop subsequent to it both taking place at Monte Verita. You are cordially invited to inform yourself on the venue, register for it and submit your scientific contributions in the fields of physico-chemical applications in pharmacy.


2.2 NEWS @

Election of the new Board of Directors

The new Board of Directors of the European Society for Applied Physical Chemistry for the years 2002 to 2004 has been elected at the General Assembly on the Munich Meeting in September:

President Board Members 
Dr. Erwin Marti Prof. Dr. Anthony E. Beezer
Vice President Dr. Elena Boldyreva
Dr. Wolf-Dieter Emmerich Dr. Katrin Fiebich
Vice President Dr. Daniéle Giron
Prof. Dr. Jean-Pierre Grolier Prof. Dr. Ulrich Griesser
General Secretary Dr. Urs Ch. Hofmeier
Prof. Dr. Emmerich Wilhelm Dr. Samuel Petit
Prof. Dr. Armin Reller


PhandTA 6, 

the 6thInternational Conference on Pharmacy and Applied Physical Chemistry of eurostar-science, takes place from Sunday, May 26 to Thursday, May 30, 2002, after PhandTA 3 in 1997 the second time @ Monte Veritá in Ascona, Switzerland. It will be followed by a one-day Workshop on theoretical and experimental aspects of the solid state  and production pathways of drug substances. The aim of the venue is to assemble scientists and specialists from universities, scientific institutes as well from research and development of the pharmaceutical industry. The anticipated subjects are in the interacting fields of Applied Physical Chemistry with Pharmacy and overlap with phenomena typical also for agrochemical and food products.You may find all information on this event on the conference website, e.g.:

- the Organizing and Scientific Committee
- the
- details for
registration for participation and contributions
- accomodation
- the Workshop on Thursday, May 30, 2002

Furthermore you may register for our eNewsticker that will inform you from December 2001 on periodically about relevant news and changes, i.e. details concerning the program and the organization.



New services @ the website

We have implemented a Marketplace giving the opportunity to offer or look for special items. 
Currently eurostar-science gives several copies of the Journal of Thermal Analysis and Calorimetry, Vol. 57 (1999) to interested scientists.

Visit the Useful Link Section and the Event Schedule. Contributions to be sent to the webmaster are appreciated.




Systag AG New Reaction Calorimeter for true non-isothermal one- and two-phase systems
Netzsch GmbH Extended product portfolio due to acquisition of Holometrix Micromet, Boston, USA 
4th SELBer KopplungsTage have met all expectations ! 
TA Instruments  Basics and application of Modulated DSC in Alzenau/Aschaffenburg (D) Nov. 29 - 30, 2001
Thermal Analysis in Car Industry in Würzburg (D) Jan. 31 - Feb 01, 2002 
Solvias AG Third customer's prospect issued
Seminar on Process Analytics, November 21, 2001 in Basel 


2.3 Highlights of the Conference on 
      "Thermal Analysis and Material Science" in Munich

        Erwin Marti

Munich, September 10-13, 2001
BMW GROUP Centre for Research and Engineering (FIZ)

The Conference has been organised by three Societies from Germany and Switzerland with the goal of interactions and discussions between industry and academia. The Society eurostar-science promotes such interrelations since 1992 with seven conferences in Europe.

One group of lecturers presented reviews about development projects for new materials, composites, multifunctional compounds, polymers and additives. Another group of lecturers gave inside views about specific production processes mainly for new materials. The third group has been dealing with analytical procedures and methods applied to the characterisation of materials and substances. Most of the poster presentations pointed to specific experimental results, to evaluation methods of analytical data and also to methodological aspects.

The NETZSCH-GEFTA Award has been dedicated to Marek Maciejewski for the development of the Pulse Thermal Analysis (Pulse TA ®), a procedure which allows a variety of analytical measurements and physicochemical investigations. Examples are the calibration for a specific molecule or a group of molecules for mass spectrometers, especially also of DTA-TG-MS and TG-FTIR. Quantitative spectroscopic measurements are performed with comfortable handling. Gas - solid reactions can be studied with this procedure as a screening method for catalytic reactions and also processes of chemisorption and physisorption are straightforward elucidated.
The Award has been presented to Marek Maciejewski at the Opening Ceremony of the Conference by Michael Feist, Humboldt-University, Berlin and Wolf-Dieter Emmerich, NETZSCH Gerätebau GmbH, Selb.

Aspects of new materials and their characterisation on the basis of C/C-SiC with applications for vehicles used in the aerospace and in the stratosphere had been outlined by M. Friess, Deutsches Zentrum für Luft- und Raumfahrt, Stuttgart, and also by H. -P. Maier and G. Neuer, University of Stuttgart. Additional applications of these materials are existing also for high temperature exposures in industry.

Multifunctional, laminated, metallic materials processed by thixoforming at high temperatures around 1400°C in partially liquid metallic phases are revealing for well-selected alloys extremely high values for the heat conductivity. Surface protection for chemical and tribological degradation processes can be achieved with ceramic layers. Th. Horning, RWTH Aachen, has presented the project, which is carried out in cooperation with several institutes. The characterisation of these materials by thermal analysis was a main point of this lecture.

Intensity modulated light sources can be used to gain valuable data about the surface properties of thin surface layers in respect to heat conductivity and to temperature gradients even in dimensions of a few micrometers. Substance inhomogeneities or mechanical distortions at the surface of materials can be made visible. The observable depth of the layers can be adjusted by changing the modulation frequency. M. Rohde, Forschungszentrum Karlsruhe, Eggenstein, has demonstrated the development of this method and he discussed selected examples.

R. Hässler, Institute for Polymer Research, Dresden, was an invited lecturer of the European Society for Applied Physical Chemistry. He presented a microthermal method (μTA ™) which combines an atomic force microscope with a thermoanalytical device, similar to a DTA or to a TMA. The instruments enable a study of surface properties with a high geometric resolution and in dimensions of a few micrometers. Some examples for laminated materials were outlined.

M. Oechsle of dmc2 , Hanau gave a review about Platiline ®, a product with applications in the area of catalytic processes as well as for moulding processes such as for glasses with high surface qualities. Additional benefits in the use of Platiline ® are the lower amount of capital bound in the production processes and the possibility of recycling the platinum.

Investigations about temperature stress and UV-irradiation applied to samples of polyoxy-methylene (POM), have been outlined by Mrs. V.-M. Archodoulaki, University of Technology, Vienna. The material is broadly used in indoor applications of cars. Screening tests, e.g. oven-storage and the Xenon test were applied to study the stability in processing and application. Additionally, different thermoanalytical methods revealed a high sensitivity for the investigation of the degradation compared with the screening methods applied.

The Institute for Ecological Chemistry, Neuherberg (München), was presented with several research activities, namely analytical investigations about additives, stabilizers and flame retardants. Qualitative and quantitative results for different groups of additives and polymers were outlined by A.A. Kettrup, G. Matuschek, and N. Milanov.

Immersion painting by electrolysis and the consecutive tempering process are production pathways of choice in the car industry. The characterisation of painting systems and the study of the kinetic reactions during tempering are straightforward achieved with measurements using DSC, DTA, DMA, TG, and TG-FTIR instruments. An insight view of the development work by the BMW Group in Dingolfing has been outlined by Ch. Froschauer. 

Additional information about the tempering process of these painting systems in laboratory experiments has been discussed. The importance of applying software programs, namely KINETIK®, ChemRheo ®, and VPS/DRY for such a development had been outlined. The cross-linking process of the varnish and the geometrical distribution of temperature-time situation over the whole car chassis were visualised with colour changing sequences. Mrs. Lang, CAD-FEM GmbH, Grafing (München) and J. Opfermann, Netzsch Gerätebau GmbH, Selb presented the interesting development work.

The synthesis and thermodynamic characterisation of polymer materials performed with a reaction calorimeter called High Pressure Scanning Transitometry (HPST) has been reported by J. -P.E. Grolier, University Blaise Pascal, Aubière, France. Professor Grolier has been an invited lecturer by the European Society for Applied Physical Chemistry. The reaction calorimeter is an instrument as well as a reactor. Temperature, pressure, and volume can be changed and by this way the heat capacities, the enthalpy changes, the compressibility, and the expansivity are determined of a given sample. Another route enables the synthesis of new materials. An example has been outlined for the high-pressure production of a polymeric material with a rather small distribution of the molecular weight. The development of taylor-made polymers by the variety of the independent parameters and the vast variation of the reactor instrument used is straightforward achieved with this reaction calorimeter.

Mrs. U. Bentrup illuminated the oxidation process of substituted aromatic compounds such as p-methoxytoluene on a V2O5 catalyst and also on phases of the formula MxV2O5-x with M as an alkali metal. The adsorption on the surface of the catalysts and its reactivity has been studied with TG, DTA, and mass spectroscopy.

The characterisation of partially crystalline thermoplastic materials using among other methods dynamic mechanical thermal analysis and temperature modulated DSC (TMDSC) has been demonstrated by Ch. Schick, University of Rostock. Step Scan DSC as an additionally development has been explained, a method which had been introduced many years ago as a step-heating procedure applied for the purity measurement by DSC. TMDSC enables heat capacity measurements better than 1%. The enthalpy calibration of DSC instruments using Indium and several other reference substances - see S.M. Sarge "DSC-Calibration with materials certified by the PTB, Braunschweig" - enable also to achieve enthalpy values better than 1%.

Ch. Schick presented as an example the structural relaxation of non cross-linked interlaced molecular chains for polystyrene. Such an energetic driven relaxation can be observed in cooling an amorphous or partially amorphous sample from a high temperature into the glass transition region. Schick found at the glass transition temperature a value for the relaxation time of about 5 minutes. E. Marti reported in his lecture "Characterisation of Polymers by Thermoanalytical Methods" also for polystyrene results obtained by G. Rehage, Technical University Clausthal. Rehage measured the change of the refraction index also under isothermal conditions above and below the glass transition temperature of 89 oC. The evaluation of an approximated relaxation time gave in a good agreement with Ch. Schick a value of 10 minutes. Interesting is the fact that the molecular chains of polystyrene in an amorphous sample are revealing only 12 K under the glass transition temperature according to Rehage a relaxation time of 1 year. This finding can be explained by the drastic decrease of the mobility in the "amorphous solid state" compared to the decrease existing in the "amorphous liquid state" in appoaching the glass transition region. A similar situation is observed by the mobilty in the corresponding solid phase. An example for this mobility are  the highly different self-diffusion coefficients of water molecules in liquid water and in ice. The fact, that such measurements becoming accessible by DSC, not below the glass transition temperature, but within the glass transition region is a consequence of the extraordinary improved sensitivity of DSC. Such instrumental developments will further enlarge the frame of the main instrument of thermal analysis, namely the DSC.

In addition, several manufacturers of instruments presented and discussed the newest instrumental developments as well as evaluation procedures.
Solvias AG, Basel distributed information about the frame of the offered services and the service capabilities.

2.4 Our sponsors. Thermometric
Dan Forsström

Thermometric AB

Thermometric is a company working in the field of thermal measurements. The spearhead product is the 2277 Thermal Activity Monitor (TAM) – a highly sensitive microcalorimeter system. The principle of measuring heat flow as a function of time has made TAM to a versatile instrument with applications in a variety of fields, e.g. biology, chemistry, pharmaceuticals and materials sciences. Measurements made with TAM are easy to conduct, non-destructive and non-invasive to the sample.

Relative Humidity  Induced Phase Transitions

Isothermal microcalorimetry is a powerful tool in quality control of pharmaceutical solids. The processing of pharmaceutical solids is often associated with large changes in physical properties which may effect the behaviour of the final product. Especially in the manufacture of microcrystalline powders, much attention has been focused on such changes. A specific problem associated with micronized crystals is to detect and quantify defect structures or "amorphous" regions in solid samples. It is well known that many substances are sensitive to moisture and will re-crystallise on exposure to elevated humidity. A procedure for studying such phenomena is to change the relative humidity linearly or step-wise from a low relative humidity to a high relative humidity. Figure 1 shows the response in heat flow of a sample of lactose on exposure to a linear increase in relative humidity.

Figure 1. A lactose sample subjected to a linear increase in relative humidity from 0 to 90 % during a period of 24 hours at 25° C, Lars-Eric Briggner, Astra Draco AB.

Oxidative Stability

Oxidation of polymeric materials causes degradation and subsequent mechanical failure. The overall oxidation process which is accompanied by a weak heat flow can continuously be monitored by TAM. Measurements may be conducted in different atmospheres, e.g. moisture, nitrogen, air and oxygen. 
In order to prevent oxidation, stabilisers are commonly added to a polymer, e.g. radical scavengers and hydroperoxide decomposers. The effect of the stabilisers on the oxidation of polyamide 6 film (40 µm thick) at 120° C in air is shown in Figure 2. The efficiency of the stabiliser is manifested by a shift of the curves towards lower heat flow levels and longer times, when the amount of antioxidant is increased.

Figure 2. The effect of different amounts of Irganox 1098, i.e. a hindered 
phenolic antioxidant, on the oxidation of polyamide 6 film at 120°C in air, 
Forsström, D., Thesis, Dept. Polymer Technology, Royal Institute of Technology, Stockholm, Sweden (1999).


The heat of solution between different batches of a compound reflects variations in polymorphism, the degree of crystallinity, surface area of particles, moisture content and surface energies among others. The energy differences between polymorphs can be accurately measured using solution calorimetry and the different physical forms and their mixtures can be identified. Many solid drug formulations exhibit wetting and swelling characteristics that can be studied by exposing the solids to solvent. In this case the energetics of the solid/liquid interaction is obtained. Figure 3 shows the heat of solution of different polymorphs in acetone and DMF.

Figure 3. Heat of Solution of two polymorphs in Acetone and DMF, S.Lindenbaum and S. E. McGraw, Pharmaceutical Manufacturing, Jan 1985.


Isothermal Titration Calorimetry

Molecular interactions are defined by stochiometry and a few thermodynamic parameters. Procedures such as equilibrium dialysis are time consuming, require large amount of materials and good results are often difficult to achieve. Since binding reactions generate heat, calorimetry greatly simplifies the methodology. One reactant is placed within the calorimeter and titrated with the second. The heat flow (and heat) associated with each injection is continuously measured. An experiment can be completed within hours. Titration Calorimetry adds an understanding of the energetics of a target system and gives structural related information. The technique offers a secondary screening assay and is valuable in the iterative rational drug design process. Figure 4 shows a typical response in heat flow during a titration experiment.

Figure 4. Typical response in heat flow during an isothermal titration calorimetric experiment.

Amorphicity and Crystallinity

Micronisation and other processing techniques can cause changes in the crystallinity of solids. It is often important to know the proportion of amorphous phase present. Within the TAM it is possible to induce recrystallisation of the amorphous content back to crystalline. This process is highly energetic and can be used to quantify the amount of amorphous product present in the initial sample. By using this method it is possible to detect levels well below 1% amorphicity within a sample. Figure 5 shows the response in heat flow of different samples of Cefadroxil when exposed to 100 % relative humidity.

Figure 5. Sorption of 100% relative humidity onto different 
samples of Cefadroxil, Lehto and Laine, Int. J. Pharm. 163, 49-62, 1998.

Dissolution Parameters

Drugs can exist in a variety of crystal forms. Identification and control of morphology is of major importance during manufacture and subsequent processing. Different forms of the same compound can have widely differing initial dissolution rates and dissolution enthalpies. Using Solution Calorimetry, the difference in dissolution enthalpy can be determined. It is then possible to quantitate the amount of each morphological form in a sample of unknown composition. As Solution Calorimetry allows direct and continuous measurement of the dissolution process, the dissolution rate can also be measured. Figure 6 shows the change in temperature during a dissolution experiment using solution calorimetry. The endothermic dissolution process is preceded and followed by electrical calibrations.

Figure 6. Dissolution of a 5% amorphous Lactose sample,
Hogan & Buckton, Int. J. Pharm. 207 (2000) 57-64


Thermometric AB
Spjutvägen 5A
S-175 60 Järfälla

Phone: +46 8 564 72 200
Fax: +46 8 564 72 220


Top of the page  

© eurostar-science, 2001
issued: October 14, 2001 by katiniko